Lucien jean joseph perruche



ToaZZ wh omiz't may concern Be it known that I, LUOIEN PnmmoH'E, citizen of the Republic of France,

provements are fully ing specification.

U I E -ST TESP T f Lucian Juan- .rosnrn-grnnnuonn; or sr-ennvns, munch.

" .PBOGESS m B nucrIoN or in rno comrounns.

J an: Josnrn and resident of' .St. Gervais, France (post ofiice address, 16 Rue des Coutures,) have invented anew and useful Process forvthe Production of Nitro Compounds, which im- The object of the presentinventio-n is a process for the production of aromatic nitro ditions nitrogen peroxid yields nitric acid compounds and consists in passing oxygen, ozonized air or a1r under pressure into a mixture of the substance to be' mtrated, with liquid nitrogen peroxid and traces of water under cooling.

In the presence of oxygen under these conin stcttu nascendi, according to the following equation I This nascent nitric acid reacts on the substance to, be nitrated, furnishing a nitro compound and water, which latter in turn reacts with a fresh amount of nitrogen pe-.-

froxid and oxygen with formation of nitric acid, the cycle of operations beingrepeated. The final productconsists of-a mixture of nitro compound, nitric acid -equivalent to the water set free by the nitration-and an' excess of nitrogen peroxid. The nitrogen peroxid is removed by distillation or by a' current of air, leaving a mixture of the nitro compound and of nitric acid. The nitro com ound may be separated by any suitable met 0d, or the mixture of nitrlc acid and the nitro compound may be used for the production of polynitro products, by'the action of sulfuric acid, for instance on the mixture such as it is or after the addition of a further quantity of the substance to be mtrated.

EwwmpZe 1.

The production of nitrobenzene or of metadinitrobenccne.l00 parts by weightof liquid nitrogen peroxid, parts of benzene 0 and +20 C. By the end of 6 to 10 hours the operation is completed, the exces nitrogen peroxid is removed by set forth in the followof distilllftion or bythe action of a current of hot air, and

a mixture of nitrobenzene and nitric acid re- Specification of Iette'rs ratent. Patented Dec. 16, 1919. Application filed August: 19,1918. Serial Ii'o. 250,547.

mains. The nitric acid can be neutralized by saturation. with a base such as lime, ain- 'monia and the like which gives the corresponding nitrate, the nitrobenzenebeing recovered in a pure state by distillation with V or without steam;v The m xture may -also be extracted with carbon tetrachlorid, the nitrobenzene being separated by evaporatmg the solvent.

he mixture cf nitric acid and nitroben- 'zen'e may also be treated with sulfuric acid,

heated andvprecipitated by waterir. order to produce dmitrobenzene. v

This operation can be efiected in the presonly purpose of using higher pressure bein ence of oxygen-at ordinary pressure, the I to accelerate the reaction. When air is use, I

. however, the'reaction' must be carried out under pressure. Ewai pie 2.

' Production of art 0 and para mtroa/nis0Z.-l0 parts by weight of-anisol dissolved in 50 parts of carbon tetrachlorid are poured into an autoclave.

(The carbon tetrachlorid is used to moderate the violence of the I reaction). kept cooled between 0 and {20 (1,50 parts of liquid nitrogen peroxid are added, followed by treatment with compressed air or oxygen at about 5 kilos. per sq.cm. during about 20 hours. The pressure may be varied; the higher the pressure the more ra id the reaction.

he excess of nitrogen peroxid is removed by distillation or by means of a' current of hot air, and in order to separate the nitroanisol the 'mixture' is treated. either with water or a base or additional carbon tetra- Thereupon, the; mixture being chlorid. The nitroanisol consists of a mix- I .ture of orthonitroanisol and paranitroanisol which are'separated by the usual methods.

Under these conditions about 30% orthoand- 70% para product are obtained.

What I claim as new and desire to secure byv Letters Patent of the United States is v 1. In a process of producing aromatic nitro compounds, the herein described steps of mixing the substance to be nitrated with liquid nitrogen peroxid; passing an oxidiz-. f

of mixing the substance to be nitrated with liquid nitrogen peroxid and traces of water; and then passing an oxidizing agent into the mixture. 7

3. In a process of producing aromatic nitro compounds, the herein described steps of mixing the substance to be nitrated with liquid nitrogen peroxid and traces of water; and then passing an oxidizing agent into the mixture ,while maintaining it under pressure.

4. In a process of producing aromatic nitro compounds, the herein described steps of mixing thesubstanc to be nitrated with liquid nitrogen peroxid; passing an oxidizing agent into the mixture; and then re1n0ving the excess nitrogen peroxid, leaving a' passing an oxidizing agent into the mixture cooling the mixture; and then removing the excess nltrogen peroxld, leaving a mixture of nitric acid and a nitro compound.

In testimony whereof I have si ed this specification 1n the presence of a su scribing witness.

Luann: JEAN JOSEPH PERRUGHE.

Witness:

JOHN F. S1MoNs.-- 

